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The title compound is built from edge-sharing centrosymmetric dimeric [Zr2F12]4− complexes, HF mol­ecules, Rb+ and K+ cations. Rubidium and potassium ions are statistically disordered on one of the metal positions. The ZrIV coordination polyhedron is a monocapped trigonal prism. The two crystallographically independent Rb(K) ions are coordinated by F atoms and HF mol­ecules with coordination numbers 7 and 9, respectively, for the two sites. In addition, the structure is stabilized by strong F—H...F hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807058278/fi2047sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807058278/fi2047Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](r-F) = 0.001 Å
  • Disorder in main residue
  • R factor = 0.026
  • wR factor = 0.061
  • Data-to-parameter ratio = 20.5

checkCIF/PLATON results

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Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? PLAT301_ALERT_3_C Main Residue Disorder ......................... 14.00 Perc.
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

This work is a continuation of the study of the structure and physicochemical properties of zirconium fluoride complexes with homo- and heteroatomic cations (Gerasimenko et al., 2006, 2007a, 2007b; Kavun et al., 2006) and deals with synthesis and crystal structure of rubidium–potassium hexafluoridozirconate(IV) di(hydrogen fluoride), Rb2 - xKxZrF6·2HF (I) where x=0.4171. The asymmetric unit contains one Zr atom, six fluorine atoms, two sites of rubidium and potassium cations and two hydrogen fluoride molecules. The Zr atoms are coordinated by seven F atoms in a slightly distorted monocapped trigonal prism geometry. Two Zr-centred polyhedra are linked by double F bridges to form a centrosymmetric dimeric [Zr2F12]4- complex (Fig. 1) with a Zr···Zri distance of 3.6579 (4) Å. Along to the c direction, Zr- polyhedra pack up in columns (Fig. 2).

In this structure, there are two sites in which the outer-sphere rubidium and potassium cations are located. In each site the rubidium cations are statistically substituted by the potassium cations. According to the performed refinement, Rb/K site occupancy factors are equal to 0.8742 (7)/0.1258 for the Rb1/K1 site and 0.7087 (7)/0.2913 for the Rb2/K2 site. The coordination numbers (CN) of these sites were calculated by the method of intersecting spheres (Serezhkin et al., 1997) with use of the program package TOPOS (Blatov, 2004). For the first site (Fig. 3a), the CN is 9 (Rb1(K1)–F, 2.7609 (14) – 3.1054 (13) Å) and for the second site (Fig. 3 b), the CN is 7 (Rb2(K2)–F, 2.7584 (14) – 2.9094 (14) Å).

The HF molecules are involved as donors in strong hydrogen bonds (2.326 (2), 2.402 (2) and 2.326 (8) Å) with the F6ii and F4 atoms (Fig. 2). The F8 atom of HF molecule is split on two sites: F8a and F8b (Fig. 2, 3). The refined occupancy of the F8a and F8b sites are 0.790 (4) and 0.210 (4), respectively. Unfortunately, we did not manage to split the position of H2 atom, therefore, the angle of the hydrogen bond F8b–H2···F4 equal to139(4)° is unusual for strong hydrogen bonds.

Related literature top

For related literature, see: Blatov (2004); Gerasimenko et al. (2006), Gerasimenko, Didenko & Kavun (2007); Gerasimenko, Kavun et al. (2007); Kavun et al. (2006); Serezhkin et al. (1997).

Experimental top

ZrO2 (6.2 g, 0.05 mol; Reachem(Russia), 99.99% purity) was reacted with RbF (7.8 g, 0.075 mol; Alfa Aesar, 99.7% purity) and KF·2H2O (2.4 g, 0.025 mol; Reachem(Russia), 99.99% purity) in a solution of hydrofluoric acid (40%, 30 ml; Reachem(Russia), 99.99% purity). Upon slow evaporation at room temperature, crystals of Rb5 - xKxZr3F17·0.5H2O (x =2.0 and 2.25) precipitated first (later we will report about their crystal structures), and after they were separated, crystals of (I) precipitated next.

Refinement top

The Rb and K site occupancies were refined together with the refinement of the structural parameters of these atoms, assuming that their positional and thermal parameters were the same. The site-occupancy factors of F8a and F8b atoms were refined by restraining the sum of occupancies to 1.0. Their displacement parameters were constrained to be identical using the EADP instructions. The H atoms were found in a difference Fourier map and refined with Uiso(H) = 1.5Ueq(F). The maximum peak and deepest hole are located 0.79 Å and 0.72 Å, respectively, from Zr and F6.

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXTL (Bruker, 1998); program(s) used to refine structure: SHELXTL (Bruker, 1998); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL (Bruker, 1998).

Figures top
[Figure 1] Fig. 1. A view of the centrosymmetric dimeric [Zr2F12]4- complex, with displacement ellipsoids drawn at the 50% probability level. Symmetry code as in Table 1.
[Figure 2] Fig. 2. The structure of (I), viewed along the c axis.
[Figure 3] Fig. 3. (a) The Rb1(K1) and (b) Rb2(K2) coordination polyhedra, with displacement ellipsoids drawn at the 50% probability level. Symmetry codes: ii: 1 - x, 1/2 + y, 1/2 - z; iv: 1 - x, 2 - y, -z; v: 1 - x, -1/2 + y, 1/2 - z; vi: 1 + x, 3/2 - y, -1/2 + z; vii: 1 + x, y, z; ix: x, -1 + y, z; x: 1 + x, -1 + y, z; xii: 1 - x, 1 - y, z.
Rubidium potassium hexafluoridozirconate(IV) bis(hydrogen fluoride) top
Crystal data top
Rb1.58K0.42ZrF6·2HFF(000) = 722
Mr = 396.84Dx = 3.425 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 1764 reflections
a = 7.2427 (5) Åθ = 2.8–31.3°
b = 11.7111 (8) ŵ = 11.68 mm1
c = 9.0742 (6) ÅT = 173 K
β = 90.413 (2)°Prism, colourless
V = 769.65 (9) Å30.27 × 0.22 × 0.17 mm
Z = 4
Data collection top
Bruker SMART 1000 CCD area-detector
diffractometer
2437 independent reflections
Radiation source: fine-focus sealed tube2223 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
Detector resolution: 8.33 pixels mm-1θmax = 31.5°, θmin = 2.8°
ω scansh = 1010
Absorption correction: gaussian
(SADABS and XPREP; Bruker, 2003)
k = 1716
Tmin = 0.176, Tmax = 0.444l = 137
6082 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.026Only H-atom coordinates refined
wR(F2) = 0.061 w = 1/[σ2(Fo2) + (0.0216P)2 + 0.8571P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.026
2437 reflectionsΔρmax = 0.68 e Å3
119 parametersΔρmin = 0.62 e Å3
1 restraintExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0034 (3)
Crystal data top
Rb1.58K0.42ZrF6·2HFV = 769.65 (9) Å3
Mr = 396.84Z = 4
Monoclinic, P21/cMo Kα radiation
a = 7.2427 (5) ŵ = 11.68 mm1
b = 11.7111 (8) ÅT = 173 K
c = 9.0742 (6) Å0.27 × 0.22 × 0.17 mm
β = 90.413 (2)°
Data collection top
Bruker SMART 1000 CCD area-detector
diffractometer
2437 independent reflections
Absorption correction: gaussian
(SADABS and XPREP; Bruker, 2003)
2223 reflections with I > 2σ(I)
Tmin = 0.176, Tmax = 0.444Rint = 0.033
6082 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0261 restraint
wR(F2) = 0.061Only H-atom coordinates refined
S = 1.06Δρmax = 0.68 e Å3
2437 reflectionsΔρmin = 0.62 e Å3
119 parameters
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr0.13506 (2)0.979721 (14)0.169058 (18)0.01248 (4)
Rb10.85934 (3)0.681632 (16)0.00920 (2)0.01949 (5)0.8742 (7)
K10.85934 (3)0.681632 (16)0.00920 (2)0.01949 (5)0.1258
Rb20.63267 (3)0.14738 (2)0.22385 (2)0.02009 (6)0.7087 (7)
K20.63267 (3)0.14738 (2)0.22385 (2)0.02009 (6)0.2913
F20.05205 (17)1.02431 (10)0.31821 (13)0.0210 (3)
F10.05701 (15)0.91307 (9)0.04199 (12)0.0172 (2)
F50.08382 (18)0.81754 (10)0.22501 (13)0.0232 (3)
F60.2991 (2)0.97382 (11)0.36010 (14)0.0300 (3)
F30.25829 (19)1.13146 (11)0.16978 (18)0.0335 (3)
F40.37882 (18)0.92093 (14)0.08435 (16)0.0360 (4)
F70.5434 (2)0.17326 (12)0.52128 (18)0.0402 (4)
H10.593 (5)0.121 (3)0.560 (4)0.060*
F8a0.6904 (3)0.8804 (2)0.1602 (3)0.0417 (6)0.790 (4)
F8b0.6467 (11)0.8442 (8)0.1869 (10)0.040 (2)0.210 (4)
H20.586 (5)0.897 (3)0.147 (4)0.060*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zr0.01345 (7)0.01337 (7)0.01059 (7)0.00168 (6)0.00099 (6)0.00001 (6)
Rb10.02571 (10)0.01514 (8)0.01765 (9)0.00183 (7)0.00263 (7)0.00237 (6)
K10.02571 (10)0.01514 (8)0.01765 (9)0.00183 (7)0.00263 (7)0.00237 (6)
Rb20.01561 (10)0.02453 (11)0.02013 (11)0.00128 (8)0.00099 (8)0.00070 (8)
K20.01561 (10)0.02453 (11)0.02013 (11)0.00128 (8)0.00099 (8)0.00070 (8)
F20.0253 (6)0.0220 (5)0.0156 (5)0.0044 (4)0.0042 (4)0.0006 (4)
F10.0210 (5)0.0169 (5)0.0138 (5)0.0053 (4)0.0029 (4)0.0029 (4)
F50.0330 (6)0.0160 (5)0.0207 (6)0.0031 (4)0.0029 (5)0.0033 (4)
F60.0370 (7)0.0303 (6)0.0226 (6)0.0114 (5)0.0128 (5)0.0042 (5)
F30.0259 (6)0.0244 (6)0.0501 (8)0.0088 (5)0.0119 (6)0.0105 (6)
F40.0154 (5)0.0602 (9)0.0324 (7)0.0094 (6)0.0016 (5)0.0153 (6)
F70.0547 (9)0.0300 (7)0.0359 (8)0.0137 (6)0.0158 (7)0.0032 (6)
F8a0.0205 (8)0.0497 (12)0.0547 (13)0.0074 (8)0.0132 (8)0.0072 (10)
F8b0.027 (4)0.052 (5)0.040 (4)0.015 (3)0.012 (3)0.002 (3)
Geometric parameters (Å, º) top
Zr—F31.9886 (13)F1—Zri2.1950 (11)
Zr—F21.9919 (12)F1—K2xii2.8860 (11)
Zr—F52.0014 (11)F1—Rb2xii2.8860 (11)
Zr—F42.0497 (13)F1—Rb1xiv3.0806 (11)
Zr—F62.0958 (13)F1—K1xiv3.0806 (11)
Zr—F12.1403 (11)F5—K2ii2.8964 (12)
Zr—F1i2.1950 (11)F5—Rb2ii2.8964 (12)
Zr—Zri3.6579 (4)F5—Rb1iii2.9183 (12)
Zr—K1ii3.8882 (3)F5—K1iii2.9183 (12)
Zr—Rb1ii3.8882 (3)F5—Rb1xiv3.1054 (13)
Zr—K1iii4.0207 (3)F5—K1xiv3.1054 (13)
Zr—Rb1iii4.0207 (3)F6—K1ii3.0156 (13)
Rb1—F3iv2.7609 (14)F6—Rb1ii3.0156 (13)
Rb1—F2v2.8829 (12)F6—K2xv3.3969 (15)
Rb1—F5vi2.9183 (13)F6—Rb2xv3.3969 (15)
Rb1—F7ii2.9197 (18)F3—K2xv2.7584 (14)
Rb1—F2vi2.9489 (12)F3—Rb2xv2.7584 (14)
Rb1—F6v3.0156 (13)F3—Rb1iv2.7609 (14)
Rb1—F8b3.033 (9)F3—K1iv2.7609 (14)
Rb1—F8a3.051 (2)F3—K1ii3.2550 (16)
Rb1—F1vii3.0806 (11)F3—Rb1ii3.2550 (16)
Rb1—F5vii3.1054 (13)F4—K2xii2.9094 (14)
Rb1—F8bviii3.164 (9)F4—Rb2xii2.9094 (14)
Rb1—F3v3.2550 (16)F4—Rb2xv3.4615 (16)
Rb2—F3ix2.7584 (14)F7—K2xvi2.8621 (16)
Rb2—F72.7964 (17)F7—Rb2xvi2.8621 (16)
Rb2—F2x2.8278 (12)F7—Rb1v2.9197 (18)
Rb2—F7xi2.8621 (16)F7—K1v2.9197 (18)
Rb2—F1xii2.8860 (11)F7—H10.79 (4)
Rb2—F5v2.8964 (12)F8a—F8b0.583 (9)
Rb2—F4xii2.9094 (14)F8a—K2xv3.207 (2)
Rb2—F8bv3.176 (9)F8a—Rb2xv3.207 (2)
Rb2—F8aix3.207 (2)F8a—Rb1xvii3.313 (2)
Rb2—F6ix3.3969 (15)F8a—K1xvii3.313 (2)
Rb2—F4ix3.4615 (16)F8a—H20.79 (4)
Rb2—F8bix3.568 (9)F8b—K1xvii3.164 (9)
F2—K2xiii2.8278 (12)F8b—Rb1xvii3.164 (9)
F2—Rb2xiii2.8278 (12)F8b—K2ii3.176 (9)
F2—Rb1ii2.8829 (12)F8b—Rb2ii3.176 (9)
F2—K1ii2.8829 (12)F8b—Rb2xv3.568 (9)
F2—K1iii2.9489 (12)F8b—H20.84 (4)
F2—Rb1iii2.9489 (12)
F3—Zr—F294.07 (6)F8bv—Rb2—F6ix83.42 (16)
F3—Zr—F5158.63 (6)F8aix—Rb2—F6ix64.92 (4)
F2—Zr—F587.03 (5)F3ix—Rb2—F4ix50.53 (4)
F3—Zr—F485.05 (6)F7—Rb2—F4ix108.06 (4)
F2—Zr—F4159.22 (5)F2x—Rb2—F4ix98.39 (3)
F5—Zr—F486.46 (6)F7xi—Rb2—F4ix102.15 (4)
F3—Zr—F677.00 (6)F1xii—Rb2—F4ix90.96 (3)
F2—Zr—F680.28 (5)F5v—Rb2—F4ix163.69 (3)
F5—Zr—F682.18 (5)F4xii—Rb2—F4ix55.00 (5)
F4—Zr—F679.30 (6)F8bv—Rb2—F4ix108.15 (15)
F3—Zr—F1116.39 (6)F8aix—Rb2—F4ix42.00 (4)
F2—Zr—F1121.80 (5)F6ix—Rb2—F4ix45.37 (3)
F5—Zr—F180.36 (5)F3ix—Rb2—F8bix86.82 (13)
F4—Zr—F176.38 (5)F7—Rb2—F8bix101.86 (15)
F6—Zr—F1150.76 (5)F2x—Rb2—F8bix59.86 (13)
F3—Zr—F1i76.90 (5)F7xi—Rb2—F8bix132.56 (15)
F2—Zr—F1i77.01 (4)F1xii—Rb2—F8bix71.30 (14)
F5—Zr—F1i123.92 (5)F5v—Rb2—F8bix132.78 (13)
F4—Zr—F1i122.65 (5)F4xii—Rb2—F8bix68.69 (15)
F6—Zr—F1i143.78 (5)F8bv—Rb2—F8bix139.89 (13)
F1—Zr—F1i64.93 (5)F8aix—Rb2—F8bix7.76 (14)
F3—Zr—Zri97.13 (4)F6ix—Rb2—F8bix57.28 (14)
F2—Zr—Zri99.99 (4)F4ix—Rb2—F8bix38.61 (13)
F5—Zr—Zri103.71 (4)F3ix—Rb2—H194.1 (7)
F4—Zr—Zri100.72 (4)F7—Rb2—H114.4 (7)
F6—Zr—Zri174.11 (4)F2x—Rb2—H174.3 (7)
F1—Zr—Zri32.93 (3)F7xi—Rb2—H1133.4 (7)
F1i—Zr—Zri32.00 (3)F1xii—Rb2—H1128.3 (7)
F3—Zr—K1ii56.76 (5)F5v—Rb2—H188.8 (7)
F2—Zr—K1ii45.93 (4)F4xii—Rb2—H1157.3 (7)
F5—Zr—K1ii112.13 (4)F8bv—Rb2—H175.9 (7)
F4—Zr—K1ii119.86 (4)F8aix—Rb2—H195.5 (7)
F6—Zr—K1ii50.27 (4)F6ix—Rb2—H160.6 (7)
F1—Zr—K1ii158.95 (3)F4ix—Rb2—H1103.5 (7)
F1i—Zr—K1ii94.13 (3)F8bix—Rb2—H189.9 (7)
Zri—Zr—K1ii126.108 (8)Zr—F2—K2xiii118.67 (5)
F3—Zr—Rb1ii56.76 (5)Zr—F2—Rb2xiii118.67 (5)
F2—Zr—Rb1ii45.93 (4)Zr—F2—Rb1ii104.31 (5)
F5—Zr—Rb1ii112.13 (4)K2xiii—F2—Rb1ii104.05 (4)
F4—Zr—Rb1ii119.86 (4)Rb2xiii—F2—Rb1ii104.05 (4)
F6—Zr—Rb1ii50.27 (4)Zr—F2—K1ii104.31 (5)
F1—Zr—Rb1ii158.95 (3)K2xiii—F2—K1ii104.05 (4)
F1i—Zr—Rb1ii94.13 (3)Rb2xiii—F2—K1ii104.05 (4)
Zri—Zr—Rb1ii126.108 (8)Zr—F2—K1iii107.35 (5)
K1ii—Zr—Rb1ii0.000 (4)K2xiii—F2—K1iii113.54 (4)
F3—Zr—K1iii130.00 (5)Rb2xiii—F2—K1iii113.54 (4)
F2—Zr—K1iii44.43 (3)Rb1ii—F2—K1iii108.04 (4)
F5—Zr—K1iii43.60 (4)K1ii—F2—K1iii108.04 (4)
F4—Zr—K1iii123.24 (5)Zr—F2—Rb1iii107.35 (5)
F6—Zr—K1iii70.46 (4)K2xiii—F2—Rb1iii113.54 (4)
F1—Zr—K1iii110.42 (3)Rb2xiii—F2—Rb1iii113.54 (4)
F1i—Zr—K1iii109.51 (3)Rb1ii—F2—Rb1iii108.04 (4)
Zri—Zr—K1iii113.868 (8)K1ii—F2—Rb1iii108.04 (4)
K1ii—Zr—K1iii73.249 (7)Zr—F1—Zri115.07 (5)
Rb1ii—Zr—K1iii73.249 (7)Zr—F1—K2xii113.54 (4)
F3—Zr—Rb1iii130.00 (5)Zri—F1—K2xii109.46 (4)
F2—Zr—Rb1iii44.43 (3)Zr—F1—Rb2xii113.54 (4)
F5—Zr—Rb1iii43.60 (4)Zri—F1—Rb2xii109.46 (4)
F4—Zr—Rb1iii123.24 (5)Zr—F1—Rb1xiv110.76 (4)
F6—Zr—Rb1iii70.46 (4)Zri—F1—Rb1xiv105.12 (4)
F1—Zr—Rb1iii110.42 (3)K2xii—F1—Rb1xiv101.76 (3)
F1i—Zr—Rb1iii109.51 (3)Rb2xii—F1—Rb1xiv101.76 (3)
Zri—Zr—Rb1iii113.868 (8)Zr—F1—K1xiv110.76 (4)
K1ii—Zr—Rb1iii73.249 (7)Zri—F1—K1xiv105.12 (4)
Rb1ii—Zr—Rb1iii73.249 (7)K2xii—F1—K1xiv101.76 (3)
F3iv—Rb1—F2v165.97 (4)Rb2xii—F1—K1xiv101.76 (3)
F3iv—Rb1—F5vi74.50 (4)Zr—F5—K2ii124.13 (6)
F2v—Rb1—F5vi103.22 (3)Zr—F5—Rb2ii124.13 (6)
F3iv—Rb1—F7ii72.69 (4)Zr—F5—Rb1iii108.18 (5)
F2v—Rb1—F7ii118.71 (4)K2ii—F5—Rb1iii105.57 (4)
F5vi—Rb1—F7ii122.10 (4)Rb2ii—F5—Rb1iii105.57 (4)
F3iv—Rb1—F2vi115.83 (4)Zr—F5—K1iii108.18 (5)
F2v—Rb1—F2vi71.96 (4)K2ii—F5—K1iii105.57 (4)
F5vi—Rb1—F2vi55.89 (3)Rb2ii—F5—K1iii105.57 (4)
F7ii—Rb1—F2vi100.01 (4)Zr—F5—Rb1xiv114.20 (5)
F3iv—Rb1—F6v139.43 (4)K2ii—F5—Rb1xiv97.13 (3)
F2v—Rb1—F6v53.04 (4)Rb2ii—F5—Rb1xiv97.13 (3)
F5vi—Rb1—F6v126.13 (4)Rb1iii—F5—Rb1xiv105.98 (4)
F7ii—Rb1—F6v66.82 (4)K1iii—F5—Rb1xiv105.98 (4)
F2vi—Rb1—F6v70.32 (3)Zr—F5—K1xiv114.20 (5)
F3iv—Rb1—F8b69.88 (18)K2ii—F5—K1xiv97.13 (3)
F2v—Rb1—F8b107.10 (17)Rb2ii—F5—K1xiv97.13 (3)
F5vi—Rb1—F8b140.44 (18)Rb1iii—F5—K1xiv105.98 (4)
F7ii—Rb1—F8b62.08 (17)K1iii—F5—K1xiv105.98 (4)
F2vi—Rb1—F8b159.74 (18)Zr—F6—K1ii97.42 (5)
F6v—Rb1—F8b92.68 (18)Zr—F6—Rb1ii97.42 (5)
F3iv—Rb1—F8a62.45 (6)Zr—F6—K2xv94.57 (5)
F2v—Rb1—F8a112.27 (5)K1ii—F6—K2xv87.38 (3)
F5vi—Rb1—F8a129.92 (5)Rb1ii—F6—K2xv87.38 (3)
F7ii—Rb1—F8a68.92 (5)Zr—F6—Rb2xv94.57 (5)
F2vi—Rb1—F8a168.91 (5)K1ii—F6—Rb2xv87.38 (3)
F6v—Rb1—F8a103.56 (5)Rb1ii—F6—Rb2xv87.38 (3)
F3iv—Rb1—F1vii52.65 (3)Zr—F3—K2xv120.10 (6)
F2v—Rb1—F1vii113.39 (3)Zr—F3—Rb2xv120.10 (6)
F5vi—Rb1—F1vii69.83 (3)Zr—F3—Rb1iv124.75 (6)
F7ii—Rb1—F1vii119.39 (4)K2xv—F3—Rb1iv109.85 (4)
F2vi—Rb1—F1vii124.42 (3)Rb2xv—F3—Rb1iv109.85 (4)
F6v—Rb1—F1vii158.76 (3)Zr—F3—K1iv124.75 (6)
F8b—Rb1—F1vii75.10 (18)K2xv—F3—K1iv109.85 (4)
F8a—Rb1—F1vii64.26 (5)Rb2xv—F3—K1iv109.85 (4)
F3iv—Rb1—F5vii96.48 (4)Zr—F3—K1ii92.52 (5)
F2v—Rb1—F5vii70.57 (3)K2xv—F3—K1ii94.77 (4)
F5vi—Rb1—F5vii105.77 (4)Rb2xv—F3—K1ii94.77 (4)
F7ii—Rb1—F5vii124.11 (4)Rb1iv—F3—K1ii105.93 (4)
F2vi—Rb1—F5vii131.90 (3)K1iv—F3—K1ii105.93 (4)
F6v—Rb1—F5vii107.80 (3)Zr—F3—Rb1ii92.52 (5)
F8b—Rb1—F5vii62.77 (16)K2xv—F3—Rb1ii94.77 (4)
F8a—Rb1—F5vii58.27 (4)Rb2xv—F3—Rb1ii94.77 (4)
F1vii—Rb1—F5vii51.23 (3)Rb1iv—F3—Rb1ii105.93 (4)
F3iv—Rb1—F8bviii57.94 (17)K1iv—F3—Rb1ii105.93 (4)
F2v—Rb1—F8bviii133.92 (18)Zr—F4—K2xii115.73 (6)
F5vi—Rb1—F8bviii63.29 (16)Zr—F4—Rb2xii115.73 (6)
F7ii—Rb1—F8bviii58.94 (16)Zr—F4—Rb2xv93.56 (5)
F2vi—Rb1—F8bviii64.24 (18)K2xii—F4—Rb2xv125.00 (5)
F6v—Rb1—F8bviii97.44 (16)Rb2xii—F4—Rb2xv125.00 (5)
F8b—Rb1—F8bviii109.0 (2)Rb2—F7—K2xvi130.29 (6)
F8a—Rb1—F8bviii108.51 (18)Rb2—F7—Rb2xvi130.29 (6)
F1vii—Rb1—F8bviii102.92 (16)Rb2—F7—Rb1v101.85 (5)
F5vii—Rb1—F8bviii153.48 (17)K2xvi—F7—Rb1v102.74 (5)
F3iv—Rb1—F3v124.10 (4)Rb2xvi—F7—Rb1v102.74 (5)
F2v—Rb1—F3v56.27 (3)Rb2—F7—K1v101.85 (5)
F5vi—Rb1—F3v159.03 (4)K2xvi—F7—K1v102.74 (5)
F7ii—Rb1—F3v76.19 (4)Rb2xvi—F7—K1v102.74 (5)
F2vi—Rb1—F3v114.48 (3)Rb2—F7—H1104 (3)
F6v—Rb1—F3v47.68 (3)K2xvi—F7—H1100 (3)
F8b—Rb1—F3v54.60 (18)Rb2xvi—F7—H1100 (3)
F8a—Rb1—F3v63.41 (5)Rb1v—F7—H1120 (3)
F1vii—Rb1—F3v112.03 (3)K1v—F7—H1120 (3)
F5vii—Rb1—F3v65.43 (3)F8b—F8a—Rb182.8 (9)
F8bviii—Rb1—F3v132.73 (15)F8b—F8a—K2xv124.3 (9)
F3ix—Rb2—F786.85 (5)Rb1—F8a—K2xv152.61 (8)
F3ix—Rb2—F2x144.10 (4)F8b—F8a—Rb2xv124.3 (9)
F7—Rb2—F2x87.41 (4)Rb1—F8a—Rb2xv152.61 (8)
F3ix—Rb2—F7xi73.63 (5)F8b—F8a—Rb1xvii70.3 (9)
F7—Rb2—F7xi119.18 (4)Rb1—F8a—Rb1xvii98.15 (6)
F2x—Rb2—F7xi138.31 (4)K2xv—F8a—Rb1xvii95.66 (6)
F3ix—Rb2—F1xii130.57 (4)Rb2xv—F8a—Rb1xvii95.66 (6)
F7—Rb2—F1xii139.90 (4)F8b—F8a—K1xvii70.3 (9)
F2x—Rb2—F1xii54.38 (3)Rb1—F8a—K1xvii98.15 (6)
F7xi—Rb2—F1xii89.20 (4)K2xv—F8a—K1xvii95.66 (6)
F3ix—Rb2—F5v140.34 (4)Rb2xv—F8a—K1xvii95.66 (6)
F7—Rb2—F5v86.53 (4)F8b—F8a—H274 (3)
F2x—Rb2—F5v74.46 (4)Rb1—F8a—H2120 (3)
F7xi—Rb2—F5v75.80 (4)K2xv—F8a—H270 (3)
F1xii—Rb2—F5v72.92 (3)Rb2xv—F8a—H270 (3)
F3ix—Rb2—F4xii77.83 (4)Rb1xvii—F8a—H2123 (3)
F7—Rb2—F4xii162.24 (5)K1xvii—F8a—H2123 (3)
F2x—Rb2—F4xii99.69 (4)F8a—F8b—Rb186.2 (9)
F7xi—Rb2—F4xii65.15 (4)F8a—F8b—K1xvii99.7 (10)
F1xii—Rb2—F4xii53.12 (3)Rb1—F8b—K1xvii101.8 (2)
F5v—Rb2—F4xii111.01 (4)F8a—F8b—Rb1xvii99.7 (10)
F3ix—Rb2—F8bv57.80 (15)Rb1—F8b—Rb1xvii101.8 (2)
F7—Rb2—F8bv61.51 (17)F8a—F8b—K2ii169.4 (11)
F2x—Rb2—F8bv143.82 (16)Rb1—F8b—K2ii91.2 (2)
F7xi—Rb2—F8bv59.32 (17)K1xvii—F8b—K2ii90.9 (2)
F1xii—Rb2—F8bv145.50 (16)Rb1xvii—F8b—K2ii90.9 (2)
F5v—Rb2—F8bv84.96 (15)F8a—F8b—Rb2ii169.4 (11)
F4xii—Rb2—F8bv115.52 (16)Rb1—F8b—Rb2ii91.2 (2)
F3ix—Rb2—F8aix91.79 (5)K1xvii—F8b—Rb2ii90.9 (2)
F7—Rb2—F8aix108.11 (5)Rb1xvii—F8b—Rb2ii90.9 (2)
F2x—Rb2—F8aix56.75 (4)F8a—F8b—Rb2xv47.9 (9)
F7xi—Rb2—F8aix128.97 (5)Rb1—F8b—Rb2xv134.0 (3)
F1xii—Rb2—F8aix63.57 (4)K1xvii—F8b—Rb2xv91.6 (2)
F5v—Rb2—F8aix127.33 (4)Rb1xvii—F8b—Rb2xv91.6 (2)
F4xii—Rb2—F8aix64.00 (5)K2ii—F8b—Rb2xv132.8 (3)
F8bv—Rb2—F8aix146.87 (16)Rb2ii—F8b—Rb2xv132.8 (3)
F3ix—Rb2—F6ix47.43 (4)F8a—F8b—H265 (3)
F7—Rb2—F6ix62.84 (4)Rb1—F8b—H2118 (3)
F2x—Rb2—F6ix99.19 (3)K1xvii—F8b—H2134 (3)
F7xi—Rb2—F6ix120.99 (4)Rb1xvii—F8b—H2134 (3)
F1xii—Rb2—F6ix128.33 (3)K2ii—F8b—H2108 (3)
F5v—Rb2—F6ix149.16 (3)Rb2ii—F8b—H2108 (3)
F4xii—Rb2—F6ix99.78 (4)Rb2xv—F8b—H245 (3)
Symmetry codes: (i) x, y+2, z; (ii) x+1, y+1/2, z+1/2; (iii) x1, y+3/2, z+1/2; (iv) x+1, y+2, z; (v) x+1, y1/2, z+1/2; (vi) x+1, y+3/2, z1/2; (vii) x+1, y, z; (viii) x, y+3/2, z1/2; (ix) x, y1, z; (x) x+1, y1, z; (xi) x, y+1/2, z1/2; (xii) x+1, y+1, z; (xiii) x1, y+1, z; (xiv) x1, y, z; (xv) x, y+1, z; (xvi) x, y+1/2, z+1/2; (xvii) x, y+3/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
F7—H1···F6xviii0.79 (4)1.54 (4)2.326 (2)176 (4)
F8a—H2···F40.79 (4)1.62 (4)2.402 (2)168 (4)
F8b—H2···F40.84 (4)1.62 (4)2.326 (8)139 (4)
Symmetry code: (xviii) x+1, y+1, z+1.

Experimental details

Crystal data
Chemical formulaRb1.58K0.42ZrF6·2HF
Mr396.84
Crystal system, space groupMonoclinic, P21/c
Temperature (K)173
a, b, c (Å)7.2427 (5), 11.7111 (8), 9.0742 (6)
β (°) 90.413 (2)
V3)769.65 (9)
Z4
Radiation typeMo Kα
µ (mm1)11.68
Crystal size (mm)0.27 × 0.22 × 0.17
Data collection
DiffractometerBruker SMART 1000 CCD area-detector
diffractometer
Absorption correctionGaussian
(SADABS and XPREP; Bruker, 2003)
Tmin, Tmax0.176, 0.444
No. of measured, independent and
observed [I > 2σ(I)] reflections
6082, 2437, 2223
Rint0.033
(sin θ/λ)max1)0.735
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.061, 1.06
No. of reflections2437
No. of parameters119
No. of restraints1
H-atom treatmentOnly H-atom coordinates refined
Δρmax, Δρmin (e Å3)0.68, 0.62

Computer programs: SMART (Bruker, 1998), SAINT (Bruker, 2003), SHELXTL (Bruker, 1998).

Selected bond lengths (Å) top
Zr—F31.9886 (13)Zr—F62.0958 (13)
Zr—F21.9919 (12)Zr—F12.1403 (11)
Zr—F52.0014 (11)Zr—F1i2.1950 (11)
Zr—F42.0497 (13)Zr—Zri3.6579 (4)
Symmetry code: (i) x, y+2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
F7—H1···F6ii0.79 (4)1.54 (4)2.326 (2)176 (4)
F8a—H2···F40.79 (4)1.62 (4)2.402 (2)168 (4)
F8b—H2···F40.84 (4)1.62 (4)2.326 (8)139 (4)
Symmetry code: (ii) x+1, y+1, z+1.
 

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